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Ethanol → HCID 68285705, 화합물

HRID 1053277
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HRID 1053277 반응식
Br[C:2]1[C:6]([N:7]([CH3:9])[CH3:8])=[C:5]([C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][CH:11]=2)[S:4][C:3]=1[C:17]([O:19][CH2:20][CH3:21])=[O:18].C(O)C.[S:25]([C:29]1[CH:34]=[CH:33][C:32](B(O)O)=[CH:31][CH:30]=1)(=[O:28])(=[O:27])[NH2:26].C(=O)([O-])[O-].[K+].[K+]>C1(C)C=CC=CC=1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[Cl:16][C:13]1[CH:14]=[CH:15][C:10]([C:5]2[S:4][C:3]([C:17]([O:19][CH2:20][CH3:21])=[O:18])=[C:2]([C:32]3[CH:33]=[CH:34][C:29]([S:25](=[O:28])(=[O:27])[NH2:26])=[CH:30][CH:31]=3)[C:6]=2[N:7]([CH3:9])[CH3:8])=[CH:11][CH:12]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 702EthanolHCID 11430Potassium CarbonateHCID 223919774-(Aminosulphonyl)benzeneboronic acidHCID 68285965HCID 68285965, 화합물2회

생성물 1

HCID 68285705HCID 68285705, 화합물수율 76.1%

시약·촉매·용매 2

HCID 178418397
HCID 178418397, 화합물
촉매
HCID 1140Toluene용매

반응 조건

온도
25 °C

실험 절차

To a solution of Ethyl 3-bromo-5-(4-chlorophenyl)-4-(dimethylamino)thiophene-2-carboxylate (compound 34d, 2.20 g, 5.65 mmol) in a mixture of toluene:ethanol (10 ml:30 ml) was added (4-sulfamoylphenyl)boronic acid (1.25 g, 6.22 mmol) and potassium carbonate (1.56 g, 11.30 mmol) at 25° C. Nitrogen gas was bubbled through the reaction mixture for 15 minutes. To the reaction mixture was then added tetrakis(triphenylphosphine)palladium(0) (0.32 g, 0.28 mmol) under nitrogen and the reaction mixture was heated at about 95 to about 100° C. for 16 hr under stirring. The progress of the reaction was monitored by TLC. The reaction mixture was then cooled to 25° C. and filtered through celite. The celite cake was then washed with ethanol (2×25 ml). The combined filtrate was concentrated under reduced pressure to obtain a crude product, which was then purified by flash column chromatography using 55% ethyl acetate in hexanes as an eluent to obtain the title compound (2.0 g, 76.05%).

후처리

  1. customNitrogen gas was bubbled through the reaction mixture for 15 minutes
  2. filtrationfiltered through celite
  3. washThe celite cake was then washed with ethanol (2×25 ml)
  4. concentrationThe combined filtrate was concentrated under reduced pressure
  5. customto obtain a crude product, which
  6. customwas then purified by flash column chromatography

출처 및 근거

ORD 기록
ord-0879e9fadd6b4f91bcfaa6ad59b0fa70
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09393247B2

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